Carbon nanospheres (CNSs) with diameter of around 100 nm were synthesized by pyrolysis technique using activated carbon as Fe-catalyst support and palm oil as carbon precursors with various ratios. Firstly, the Fe catalyst were deposited onto the activated carbon by incipient wetness impregnation method using Fe(NO3)2 x 9H2O as precursors with various content of catalyst (5%, 7% and 10% with respect to the carbon support). The carbon products were characterized by X-ray diffraction, transmission electron microscope, scanning electron microscope, Raman spectroscopy, nitrogen adsorption and X-ray photoelectron spectroscopy. Preliminary electrochemical characteristics of as-synthesized CNSs as anode materials of lithium secondary batteries were conducted using Cyclic Voltammetry to observe the mechanism of Li-ion insertion/extraction during charge-discharge tests.